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Water → ethyl 4-[1-methyl-6-(pyridin-2-ylmethoxy)-1H-pyrrolo[2,3-b]pyridin-3-yl]-3-oxopiperazine-1-carboxylate

HRID 1622896
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HRID 1622896 반응식
Cl.[CH3:2][N:3]1[C:7]2=[N:8][C:9]([O:12][CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)=[CH:10][CH:11]=[C:6]2[C:5]([N:20]2[CH2:25][CH2:24][NH:23][CH2:22][C:21]2=[O:26])=[CH:4]1.C(N(CC)CC)C.[C:34](Cl)(=[O:38])[O:35][CH2:36][CH3:37].O>C(Cl)Cl.CCOCC>[CH3:2][N:3]1[C:7]2=[N:8][C:9]([O:12][CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)=[CH:10][CH:11]=[C:6]2[C:5]([N:20]2[CH2:25][CH2:24][N:23]([C:34]([O:35][CH2:36][CH3:37])=[O:38])[CH2:22][C:21]2=[O:26])=[CH:4]1
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참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 1317316621-[1-methyl-6-(pyridin-2-ylmethoxy)-1H-pyrrolo[2,3-b]pyridin-3-yl]piperazin-2-one, hydrochloride

생성물 1

HCID 67817855ethyl 4-[1-methyl-6-(pyridin-2-ylmethoxy)-1H-pyrrolo[2,3-b]pyridin-3-yl]-3-oxopiperazine-1-carboxylate수율 60.3%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-[1-methyl-6-(pyridin-2-ylmethoxy)-1H-pyrrolo[2,3-b]pyridin-3-yl]piperazin-2-one, hydrochloride (0.10 g, 0.267 mmol) and triethylamine (160 μL, 1.148 mmol) in DCM (1.5 mL) is added dropwise ethyl carbonochloridate (35 μL, 0.366 mmol) at room temperature and the reaction mixture is stirred for 1.5 h. The reaction is poured into water and extracted with DCM. After separation, the organic layer is dried over sodium sulphate, filtered and concentrated in vacuo. The residue is purified on silica gel (10 g Isolute cartridge), eluting with EtOAc, to afford a very dense pale yellow oil, which solidified upon addition of Et2O. The material is triturated in Et2O, filtered off and washed twice with Et2O, to afford the title compound (0.066 g, 0.161 mmol) as a colorless solid. MS (m/z) 410 (M+1).

후처리

  1. extractionextracted with DCM
  2. customAfter separation
  3. dry with materialthe organic layer is dried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue is purified on silica gel (10 g Isolute cartridge)
  7. washeluting with EtOAc
  8. customto afford a very dense pale yellow oil, which
  9. customThe material is triturated in Et2O
  10. filtrationfiltered off
  11. washwashed twice with Et2O

출처 및 근거

ORD 기록
ord-aa9bd7959cd54c0db49452c3a38cf22a
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08778946B2

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